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By J. S. McNeil, J. U. Messenger

In the drilling of oil wells the control and prevention of lost circulation of the drilling- fluid is a oroblem which is frequently encountered; in many cases existing materials and methods for alleviating this condition have not been adequate. For severe cases of lost circulation in which the simpler methods, such as application of various bridging materials to the mud system, have proven unsatisfactory. a new material and method for applying to the loss zones have been developed which appear to he superior to existing techniques in many respects. The material, called a clay cement, is capable of being handled as a drilling fluid after initial mixing of the solitl ingredients with water and may be pumped down the drill pipe and squeezed into loss zones. After a short period, the material develops a very high gel strength which seals off the zone against further losses of the drilling fluid. In field tests, the process has been demonstrated to be a very effective method for combatting lost circulation. INTRODUCTION Methods of treating lost circulation in rotary-drilled wells by the addition of special materials to drilling fluids have long been in the process of development and are continuing to improve.' However, the annual drilling costs which can be traced directly to lost circulation difficulties still run into the millions of dollars. The loss of mud materials into highly permeable zones may range up to $50,000 per well in some areas. In addition to mud costs, excessive requirements of casing, cement; rig time, and the attendant blowout hazards further emphasize the importance of the need for improved methods of combatting lost circulation. The shortcomings of presently-used materials and methods have led to the development of a new lost returns material in the form of a time-setting clay cement. In field tests this material has proven very successful in plugging off loss zones. which other more conventional materials had failed to do. REVIEW OF PRESENT CORRECTIVE MEASURES The proper control of such operating factors as pump pressure, clearance between pipe and hole, and speed of running pipe in a holez is of primary importance in preventing and minimizing lost circulation problems. These factors, however, concern matters of drilling technique and do not directly involve lost circulation materials. Aside from setting casing past loss zones, three principal methods are generally employed for the purpose of avoiding or combatting lost circulation: (1) adjustment in properties (principally density) of the drilling fluid, (2) addition of fibrous, flaky, granular or other types of bridging materials to the mud system, and (3) the application of cements to the loss zones. The latter method is usually employed only after the first two have proven unsuccessful. In Table I are listed some advantages and disadvantages of the common corrective measures. Frequently, a combination of bridging material and cementing material is used." This combination is based on the premise that a bridge will

Jan 1, 1952

By W. C. Ellis

Growth directions of tin, zinc, and cadmiun whisker crystals grown spontaneously fi-om the solid are summarized. In tin the edge and diagonal directions of the unit cell are jound with the exception oj- the [110] diagonal. In cadmiurn and zinc the usual dip-ections are a or a + c. The c direction has not been ohserwed. The gvouth directions from the solid are for the most part the same as those found for vapor-grozun crystals and are the ohserz:ed glide directions in plastic j-lou. Whisker crystals of these elements grown from the solid are not twinned. Specular lateral reflections are associated with planes of snall crystallographic indices. WHISKER crystals of tin, zinc, or cadmium grow spontaneously at room temperature in periods from months to years from thin electroplates and other prepared films of the respective metals.''2 It has been established that these crystals are single, but the question of twinning, such as occurs in whisker crystals of silicon,3'4 has not been resolved. Studies of morphology have been restricted to determinations of growth directions.5-' Whisker crystals are both straight and kinked. A few studies have been made on kinked whiskers including measurements of kink anglesa and determinations of growth directions,' but unfortunately not both on the same crystals. The kink angles, for the most part, for each species are grouped closely about a few unique values, but these values are not always those between observed growth directions in a single crystal. To supplement existing data, the growth directions, identification of lateral features, and presence or absence of twinning were determined with a Weissenberg goniometer by a method described elsewhereg on eight whisker crystals of tin, five of zinc, and five of cadmium. One kinked cadmium whisker was examined in detail. The specimens were needlelike, a few microns in cross section, and of the order of a millimeter in length. They were removed from electroplated substrates on laboratory specimens and commercial equipment after several years of growth as described in Table I. Since the specimens were less than 10 p in cross section they were ideally strong with no attendant risk of plastic deformation or damage in handling. Only deformation twinning has been reported for these elements. Therefore, twinning probably should not be expected in whisker crystals of these metals, particularly a twin plane containing the growth direction. A twin plane oriented in this direction was the one sought in this study. No examination was made for twinning at the boundary between kink segments except for one cadmium crystal. Well-defined reflections occur as a whisker crystal of tin, zinc, or cadmium is rotated about its growth direction when illuminated by a beam of light Although these reflections had been noted in earlier investigations, no study of them was made, probably because the earlier studies had disclosed also that

Jan 1, 1967

By J. D. Price, W. M. Bertholf

One of the chief difficulties with which the operator of a coal washing plant has been forced to contend is the handling of the very fine coal. First he has the problem of separating the fine coal from washery water. This is usually accomplished by the use of settling cones or Dorr thickeners: in either event the separated fine coal contains a high amount (40 to 80 pct) of water and, somewhat loosely, dependent upon the size of the coal particles present, may be known as sludge or slurry. His second problem is the satisfactory further dewatering of such separated sludge and/or slurry. At the coal washing plant of the Colorado Fuel and Iron Corp., washed coal from the Deister Plat-O tables is sluiced to a stationary inclined de-watering screen provided with 3/16 by 1-in. slots, and the coarse coal passing over this screen is conveyed by a Baum-type elevator and a flight-type distributing conveyor to a battery of Carpenter centrifugal driers. The fine coal and water passing through the openings of the primary dewatering screens, plus the fine coal passing through the screens of the centrifugal driers (and no small portion of which is the result of the disintegrating action of these driers) is pumped to two 30-ft Link Belt settling cones. The sludge recovered as underflow from these cones was formerly dewatered on stationary screens having 1/16 by 1-in. slots and discharged on top of the coarse washed coal in the Baum drainage conveyor; but after a relatively few hours of op eration the circulating load of fine coal on this conveyor built up to a point where it became necessary to reduce the quantity of feed to the washing tables. The original arrangement of our coal washing and dewatering equipment is shown in Fig 1. In order to regain the loss in active throughput which had been caused by this circulating load, an installation of six vibrating filters was made during the year of 1936. This resulted in an increase in normal tonnage of washed coal from 1430 to 1750 tons per 8-hr shift, a gain of slightly over 22 pct. This increase in throughput has made a very substantial decrease in the " conversion cost" per ton of washed coal. Since the vibrators were installed, we have gained about 2,000,000 tons in production, compared to what would have been produced in the same number of shifts at the former rate. Putting it in slightly different form, we have saved in the past 12 yr the cost of 1400 operating shifts in the washery. Fig 2 shows the location of the vibrating filters as applied to the original flowsheet. It will be noted that the sludge from the bottom of the settling cones is passed through a distributing box and thence to the filters. The de-watered coal from the filters is de-livered to the conveyor receiving the dried coal from the Carpenter driers.

Jan 1, 1950

By M. H. Mueller, P. A. Beck, W. P. Chernock

HARRIS introduced the term inverse pole figure for the diagrams previously used by Barrett' to represent the volume fraction p(a,ß) of material in various orientations with respect to the fiber axis in a specimen with fiber texture. The direction of the fiber axis with respect to the crystal lattice is specified by the two independent angle variables a and ß. In such a diagram p gives the fiber axis density distribution over the various crystallographic directions. The p(a,ß) may be given in a two-dimensional diagram by means of contour lines (p=con-stant) in a stereographic projection. The inverse pole figure incorporates in a single contour line diagram all the information given conventionally in pole charts for various (hkl) reflections and, therefore, it represents a considerable degree of condensation. Also, it gives this information directly in terms of the volume fraction of the specimen in various orientations, and it obviates the necessity of referring back and forth between the various pole charts in an attempt to interpret them in terms of orientations. Inverse pole figures undoubtedly represent the most adequate method for describing a texture in a quantitative manner and, at least in the case of fiber textures, this method is certainly a practicable one. Harris described1 a simple procedure for determining at least the rough outlines of a quantitative inverse pole figure. This method depends on the measurement of the intensity of X-ray reflections from various (hkl) planes lying parallel to the same specimen surface. In the case of a rod, reflections from a plane specimen surface perpendicular to the rod axis (fiber texture axis) are to be used. Harris has shown that the measured intensities I,,, reflected by crystal planes (hkl), aligned perpendicularly to the fiber axis of a specimen with unknown fiber texture, and the corresponding intensity Iu nkl from a random specimen are related to the p(a,ß) value for the unknown texture by the following equation IAkl/I°Aklw=c/c°.p(a, ß) [1] where C and C° re parameters depending on the crystal imperfections (extinction), surface preparation (e.g., thickness of oxide layer), the absorption coefficient in the specimen, effective line breadth, and instrumental factors. The values of the variables a and ß1 defining the crystal orientation, depend only on the indices hkl of the reflecting plane perpendicular to the fiber axis. Since p, as described by Harris1, is normalized in such a way that upon integration over the total orientation range its mean value is 1, the parameter C/C may be calculated approximately by the summation of Eq. l over all available X-ray reflections hkl, corresponding to a set of discrete orientations (rather than by integration over the complete range of orientations represented by the continuous variables a and ß). From the summation of Eq. 1 1/n SI AKL/I° Akl = C/C. SP(a,ß)/n is obtained where, as stated above 2p(a,ß) =1. n Therefore

Jan 1, 1959

By G. D. Gemmell

Effects of solid-sdutidn alloying with titanium, molybdenum, and tungsten at concentrations up to 10 pct on the strength of pure columbium at elevated temperatures (mainly 2000°F) have been investigated by means of creep-rupture, hot-tensile, and hot-hardness testing and recrystallization studies. ThIS paper presents some results from the initial part of a study of the effects of alloying on the high-temperature strength properties of columbium. The elevated-temperature strength characteristics of pure columbium were first studied. Binary alloys of columbium with titanium, molybdenum, and tungsten containing 1, 5, and 10 pct of the solute elements were chosen on the basis of their high melting points, their known solid solubility in columbium, and results of separate oxidation-resistance studies of columbium alloys. EXPERIMENTAL PROCEDURE All the materials used were of highest purity. A typical analysis of the columbium is shown in Table I. Compositions of the alloys are also given in Table I. To evaluate the strength properties of pure co-lumbium and the alloys at elevated temperatures, creep-rupture, hot-tensile, and hot-hardness testing was done on recrystallized material. To prepare the pure metal and the alloys for these tests, 1- 1b buttons were made in a water-cooled copper crucible, inert atmosphere, tungsten arc furnace. Tapered ingots, 3 in. long, were made from these buttons by a skull-casting technique and these were machined to 1/2 in. diam, swaged to 50 pct reduction (pure columbium at room temperature, alloys at lowest temperature possible without cracking, generally in range 1100" to 1800°F) and heated in vacuum (lo-' mm Hg) for 16 hr at 2550°F for re-crystallization and homogenization. The resulting grain diameter was 0.1 to 0.3 mm. The 10 pct Mo alloy casting was not successfully swaged at temperatures up to 1800°F without cracking and was not included in the test program. Creep-rupture testing was done at constant load in vacuum on cylindrical specimens of 0.16 in. diam, using Instron capsules. The pressure at test temperatures was less than 10-1 mm Hg. Hardneas readings taken on the test specimen before and after testing were used as a check on possible gaseous contamination. Hot tensile tests in vacuum on cylindrical specimens of 0.125 in. diam were also made with Instron equipment at a strain rate of 0.067 min.-l. Hot-hardness measurements were taken with a unit constructed at the Du Pont Experimental Station. The test piece, supported on an alumina anvil, and the molybdenum indenter shaft with sapphire tip is heated in a platinum-wound furnace. The load applied to the pyramid indenter is measured by strain gages attached to a proving ring located outside the hot zone. In the measurements reported here the load was I kg. The tester operates in a vacuum of about 10"5 mm Hg and is capable of temperatures up to 1400°C.

Jan 1, 1960

By Hugh H. Waesche

High quality quartz crystals weighing more than 50 grams are required in several important industrial applications.30,31 Primarily, they are the basic raw material for precision, electronic, frequency control components; this includes oscillators and filters in both radio and telephone services. Quartz crystals are also necessary for optical lenses and prisms in special applications requiring high ultraviolet light-transmission as in spectrographs. Quartz wedges are regular components for petrographic microscopes. The application of crystalline quartz as a transducer* in ultrasonic devices has increased in recent years despite strong competition from barium titanate and magnetostrictive [f] devices. Some quartz is fabricated into delay lines for radar. Man has valued quartz for fabrication of art objects since the dawn of history. The art forms were and are painstakingly carved and polished to form intricate figurines, bowls, statuettes, and the well-known crystal balls. The largest known ball, made of perfect quartz from Burma, is now in the National Museum in Washington. It is 12 7/8 in. in diameter and weighs 106 lb 12 oz. Clear, pure quartz chips and small crystals not meeting the electronic-grade dimensional requirements are known by the Brazilian term lasca. They are used to produce fused quartz having wide application in laboratory equipment, as special glasses, for torsion suspension in scientific instruments, and as a source material for growing large artificial quartz crystals 18,35 Electronic applications far exceed all other uses in importance so any discussion of high-quality quartz crystals must be concerned almost exclusively with those functions. Historical Background Because of their ubiquitous character and natural beauty, quartz crystals have long been of interest and known to man. They have been found among early Egyptian and Chinese art forms and the Sumerians are believed to have fashioned seals, beads, and other jewelry from quartz crystals, perhaps 5,000 years ago. Also, American Indians made arrow heads and fashioned some simple objects of different kinds. The origin of the name quartz, although of Greek derivation, is uncertain. The Greeks appropriately applied their word for frozen water or ice, krustallos, to quartz. The present-day, large-scale practical applications of quartz crystals began in 1880-1881 when Pierre and Jacques Curie reported discovery of the "piezoelectric" effect. They found this effect first in Rochelle salt, a common product of grape-wine refineries, while studying crystal symmetry. Piezoelectricity is that property found in certain crystals, including quartz, whereby electrical charges of equal and opposite sign appear on opposite parts of the crystals when they are stressed. If equal and opposite forces are applied to two opposing prism edges of a single untwinned quartz crystal a positive electrical charge will appear on one edge and a negative charge on the other. The amount of the charges will be directly proportional to the force applied. This property seems to be intimately related to pyroelectricity

Jan 1, 1960

By Andrew B. Crichton

The oft repeated statements of the United States Geological Survey and the Bureau of Mines that the coal reserves in the United States are sufficient for 3000 yr have given us all a sense of security hard to disturb. If we discount that statement 66 pct, which to the uninformed seems drastic, we would still have 1000 yr supply, and why should mortal man worry about the difference between 1000 and 3000 yr supply of coal. That is exactly the attitude which many who should be better informed have taken toward the problem. A recent brochure "How Strong is America," by the New York Herald Tribune, states there is "no end to coal * * The truth is staggering * * U. S. has enough coal to last 4000 years." What the statement actually means is that the calculator got as high as 4000 yr and decided it was pointless to go on. The President's ERP Committee on Natural Resources and others in high places continue to assure the country of our superabundance of coal. In the past few days the "Wall Street Journal" carried an item from Director Boyd of the Bureau of Mines saying that within a hundred years we would need to triple our annual coal production of 600,000,000 tons, making it 1,800,000,000 tons annually, and at that rate we had coal reserves sufficient for 1000 yr. In my humble opinion, we cannot now or ever produce 1,800,000,000 tons annually, because we do not have the reserves in the producing districts to do it. Past reckoning in geology may be, as in the Psalms, a thousand years are as yesterday, but the future must be considered more realistically, and " a thousand years" is really a "heck" of a long time. In most developed areas, mining engineers can count the coal reserves in terms of a hundred years or less, and in some important areas now producing large annual tonnages in much under fifty years. They think when they hear of thousands of years coal reserves, reference is made to distant fields and "the fields are always green far away." The estimates of our coal reserves upon which we are relying were made in 1907 under the direction of Marius R. Campbell, Director of the United States Geological Survey. It is apparent this work was not well done. It was necessarily based on rather meager data because of the little development and prospecting as of that date. There were mistakes in the correlation of seams, and they assumed the continuity of thick seams throughout large coal bearing areas where coal often did not exist. The overstatement of coal bearing areas in the Campbell figures are common. The 1907 survey includes all coals over 14 in. in thickness to a depth of 3000 it. The total coal reserves according to Campbell were 3157.2 billion tons. The production and mining losses that year would amount to 570 million tons and

Jan 1, 1949

By Norris Johnston, Carrol M. Beeson

The gravimetric-vacuum distillation method was developed to permit rapid and accurate determinations of the oil-water ratios of small samples or sands containing little oil. In addition, the samples usually are so well cleaned and so little altered by the distillation at reduced pressure that rapid estimations of other physical properties may be made with the evacuated cores. Requiring only elementary glass-blowing technique, the distilling tubes and traps used in determining oil-water ratios were easily fashioned from the usual glassware. A sketch and description are given of the necessary apparatus, including the cylindrical electrical heaters. The procedure, requiring about 40 min., consists in raising the temperature and maintaining it between 675' and 725°F. for at least 10 min. while the pressure is held between I and 2 mm. Hg. The fluids condensed in the trap (cooled by a mixture of kerosine and solid carbon dioxide) are separated in a centrifuge and the volume of water is recorded. Determination of changes in weight with an analytical balance of all parts of the apparatus permits computation of weight of oil distilled and total weight of oil recovered. Introduction In determining the oil-water ratios of core samples, distillation at atmospheric pressurel-5 has proved to be sufficiently reliable for samples containing moderate quantities of oil. Since small samples and sands with little oil are encountered, how- ever, it appeared advisable to develop a method that would be applicable under these circumstances. Thegravimetric-extraction procedure1,6-9 undoubtedly is very reliable and could be used in all tests, but the time consumed in the determination would often delay field operations. This would be especially true when dealing with tight sands or viscous oils, both of which retard the extraction process. Accordingly, the gravimetric-vacuum distillation method was developed in order to combine the good features of both of the older methods; that is, accuracy and speed. By reducing the pressure, it was found possible to perform the distillation at a temperature that permits the use of glass apparatus, all parts of which can be weighed on an analytical balance. Thus, the fluids may be removed quickly from the core, the water is readily trapped and measured, and the loss in weight of the core is easily determined. In addition, the total weight of material condensed in the distilling tube and in the trap provides a method of determining the oil-water ratio that is practically independent of the one involving the loss in weight of the sample. The use of vacuum not only permits as much accuracy as does the gravimetric-extraction process, but it actually allows an increase in speed over the atmospheric-distillation method, because of the time required to cool the metal pots from about 1200°F. between runs. More important yet, the innovation makes possible the almost immediate reporting of permeability, and saturation, which is impossible

Jan 1, 1946

By Stephen Royce

[Stephen Royce.. I .......................... E. S. Moore.. 9 .......................... E. L. Bruce.. 10 ......................... J. E. Hawley.. 11 ........................ L. M. Scofield.. I 2] STEPHEN ROYCE, * Crystal Falls, Mich.Having examined and reported upon the Steep Rock Lake property and vicinity on several occasions for clients, and having kept in touch with the operation from 1938 on, the writer offers the following discussion of the valuable paper by Messrs. Roberts and Bartley, which was so kindly prepared in response to the writer's earnest request, made as a member of the Committee on Mining Geology. ORIGIN OF THE ORES The writer wishes to express complete agreement with the authors that the origin of these deposits was replacement action by hot ascending sulphide solutions of igneous origin, gaining access via the limestone and dolomite breccia channels, and acting mainly to replace the dolomite and limestone breccia with hematite and hydrated hematite. Some replacement in adjoining greenstones and tuffs by the same solutions may also have taken place, but the latter occurrences may represent replaced iron formations originally bedded in with the volcanics. Iron formation in the same relationship to volcanics is extensively developed on the western Menominee Range of Michigan, in the Middle Huronian belts; also appears in similar relations on the Vermilion Range; and is abundantly exposed in the same stratigraphic position no farther away than the southeast arm of Steep Rock Lake itself. Furthermore, the writer's classification of drill cores, made June 11, 1938, on the prop¬erty, contains the following, for hole 8, in the original strike of the A ore body: "332-342 ore; 342-350 much-leached sugary chert with thin ferruginous slate bands." This is a typical iron formation. The ore in this first group of holes (Numbers 6 to 13, incl.) is described in the writer's 1938 notes as follows: "The ore is hard, massive hematite with some limonite, and shot through with many small vugs." The breccia forms in the float ore and in the drill samples were also noted. As a field classification this does not check badly with Professor Schwartz's microscopic work. Notes supplied by Mr. Neeland, then geologist at the exploration, show: "Hole 23 has some iron formation, not logged yet." It appears therefore that there is some iron formation at the exploration, much iron formation in similar stratigraphic position in the vicinity, and iron formation similarly located as to volcanics on the Vermilion and western Menominee Ranges. Certain of the holes, notably Holes 25 and 27, showed some specular hematites resembling those known to be formed from cherty iron formation elsewhere. Hence the writer concludes that at least a small part of the Steep Rock ores results from replacement of iron formation. By far the greater part of it is, as the authors say, clearly a replaced limestone and dolomite breccia, with the breccia outlines still preserved in much of the ore, and all of the replacement is by hot ascending waters. The authors' citation of the neighboring Atikokan pyrite, pyrrhotite and magnetite

Jan 1, 1943

By J. H. Carpenter

LMENITE, rutile, zircon, and other heavy minerals are found in small amounts in the sand that covers most of Florida. Small enriched deposits occur on the beaches and coastal dunes. One beach deposit east of Jacksonville was worked during World War I and another near Vero Beach during World War 11. Both ceased operation when the resumption of imports reduced prices. Early in World War II reduction of rutile imports made a domestic source of the mineral necessary to maintain the expansion of armaments. Explorations made near Jacksonville discovered a relatively large body of low-grade ore about 10 miles inland from the beaches. A plant installed by Rutile Mining Co. of Florida using both flotation and tables encountered difficulties because of low plant capacity and organic slimes in the ore. In 1944 Humphreys Gold Corp. solved the problem of concentrating the low-grade ore by using the newly developed Humphreys spiral concentrator and by mining with a hydraulic dredge. This combination of low cost mining and concentration permitted the plant to continue operation in competition with foreign ores when imports were resumed following the war. The success of the Jacksonville operation renewed interest in Florida as a source of titanium. An extensive survey of the state was made by E. I. du Pont de Nemours and Co., Inc., under the direction of J. L. Gillson in 1945 to 1946. Sampling was carried on by drive pipe drilling to depths of 20 to 25 ft. Encouraging values were discovered near the location of the present Trail Ridge mine, 50 miles southwest of Jacksonville, near the town of Starke. The United States Bureau of Mines was interested in exploring for heavy minerals in Florida, and on the recommendation of both the state geologist of Florida and of Du Pont geologists, drilled deeper where marginal indications were found on Trail Ridge. In 1947 it was discovered that sufficiently higher values occurred at depth to make the deposit commercial. The orebody at Trail Ridge is a long sand deposit averaging about 1 mile in width and 35 ft in depth. It is approximately 1 1/2 miles wide at the north end of the portion now being worked, tapering to a blunt point 3 miles to the south. The ore reaches a maximum depth of 65 ft near the center and feathers out into barren sand at the edges. The ground surface is relatively flat and is covered with vegetation including pine, scrub oak, palmetto, and occasionally in swampy areas, cypress. The remain of a dense woody growth underlies and marks the bottom of the Ore 'One. It is difficult to drill through this layer, but in some cases where it is less than 5 ft thick it has been possible to drive through the wood. Sand lying below is coarser than that in the ore zone and contains no values. The wood layer consists of unconsolidated carbonized fragments of branches and other forest trash associated with a considerable amount of ar-

Jan 1, 1954

By Norris Johnston, Carrol M. Beeson

The gravimetric-vacuum distillation method was developed to permit rapid and accurate determinations of the oil-water ratios of small samples or sands containing little oil. In addition, the samples usually are so well cleaned and so little altered by the distillation at reduced pressure that rapid estimations of other physical properties may be made with the evacuated cores. Requiring only elementary glass-blowing technique, the distilling tubes and traps used in determining oil-water ratios were easily fashioned from the usual glassware. A sketch and description are given of the necessary apparatus, including the cylindrical electrical heaters. The procedure, requiring about 40 min., consists in raising the temperature and maintaining it between 675' and 725°F. for at least 10 min. while the pressure is held between I and 2 mm. Hg. The fluids condensed in the trap (cooled by a mixture of kerosine and solid carbon dioxide) are separated in a centrifuge and the volume of water is recorded. Determination of changes in weight with an analytical balance of all parts of the apparatus permits computation of weight of oil distilled and total weight of oil recovered. Introduction In determining the oil-water ratios of core samples, distillation at atmospheric pressurel-5 has proved to be sufficiently reliable for samples containing moderate quantities of oil. Since small samples and sands with little oil are encountered, how- ever, it appeared advisable to develop a method that would be applicable under these circumstances. Thegravimetric-extraction procedure1,6-9 undoubtedly is very reliable and could be used in all tests, but the time consumed in the determination would often delay field operations. This would be especially true when dealing with tight sands or viscous oils, both of which retard the extraction process. Accordingly, the gravimetric-vacuum distillation method was developed in order to combine the good features of both of the older methods; that is, accuracy and speed. By reducing the pressure, it was found possible to perform the distillation at a temperature that permits the use of glass apparatus, all parts of which can be weighed on an analytical balance. Thus, the fluids may be removed quickly from the core, the water is readily trapped and measured, and the loss in weight of the core is easily determined. In addition, the total weight of material condensed in the distilling tube and in the trap provides a method of determining the oil-water ratio that is practically independent of the one involving the loss in weight of the sample. The use of vacuum not only permits as much accuracy as does the gravimetric-extraction process, but it actually allows an increase in speed over the atmospheric-distillation method, because of the time required to cool the metal pots from about 1200°F. between runs. More important yet, the innovation makes possible the almost immediate reporting of permeability, and saturation, which is impossible

Jan 1, 1946

By E. S. Machlin, C. W. Chen

THIS investigation is concerned with the origin of the intercrystalline voids and cracks formed in metals and alloys subjected to stress at elevated temperature. There have been many suggestions in the recent literature relating to this problem. Greenwood' suggested that the voids may be produced by vacancy condensation. Zener has stated that shear-stress relaxation across grain boundaries could initiate high tensile stresses at the regions blocking grain boundary slip and thereby cause the formation of cracks. Chang and Grant3 have described the formation of cracks at grain boundary triple points and have experimentally verified Zener's mechanism for the grain boundary regions in the vicinity of a triple point. Subsequent to the completion of this investigation, Gifkins4 developed a model which made use of Stroh's5 mechanism of fracturing to produce sub-microscopic fractures that subsequently grow by grain boundary slip. Chen and Machlin,6 in answer to Gifkins, described a model deduced from the present investigation, in which grain boundary slip provides both the stress to fracture at grain boundary jogs and the deformation required to separate fractured jog surfaces. The possibility of gas condensation to form intercrystalline voids and cracks is eliminated as a basic mechanism because such voids and cracks are developed in vacuum melted material containing minute amounts, if any, of gaseous impurities. In a theoretical evaluation of this problem, Machlin7 concluded that void nucleation by vacancy condensation during creep-rupture is improbable but that vacancy condensation on supercritical sized voids to produce growth is probable. This investigation was begun to evaluate the suggested mechanisms for intercrystalline fracture. In particular, in order to correlate vacancy supersaturation ratios produced in creep with those determined by Bal-luffi and Seigle8 as critical for , the nucleation of voids, specimens were obtained from the same heat of brass as used by the latter authors, through the courtesy of Dr. Seigle. The experiments conducted in this investigation fall into the following categories: 1) Brass—observation of voids produced under a variety of conditions, including creep under compression, to evaluate the mechanisms of void nucleation and growth. 2) Bicrystal experiments to check the mechanism of void nucleation deduced in this investigation. 3) Morphology of intercrystalline voids produced in a variety of metals. Each set of experiments will be described and discussed separately. Experimental Techniques A special creep-rupture test rack was constructed which made it possible to apply the stress to the specimen in a controlled atmosphere of inert gas, reducing gas, or vacuum. All the creep-rupture tests on a-brass (30 pct Zn) were conducted in nitrogen under a pressure slightly above atmospheric. Either dead weight loading or constant elongation rate loading could be applied with the load measured by means of a strain gage dynamometer. In order to obtain a coarse-grained crystal structure stable at

Jan 1, 1958

By J. W. H. Clare

An equilibrium isotherm at 550°C is given for ternary alloys rich in aluminum containing 0 to 15 wt pct Cr and 0 to 20 wt pct Mn. Phases encountered are: aluminum solid solution; stable temary compound G; and MnAl8,. In addition, a limited number of alloys were annealed at 450°C to check for differences from the 550°C isotherm. These experiments limited the composition of the G phase at 550°C and further experiments established that the G Dhase is not stable above 590 ± 1 °C. RAYNOR and Little1 established several equilibrium isotherms using aluminum-rich alloys containing up to 5 pct of the elements chromium and manganese. These isotherms showed that, in addition to an a solid solution and the two binary intermediate compounds 8 and MnAl6, a stable ternary compound ex-isted in the system. This phase was called the G phase because of its ghostly appearance in micro-sections. Little, Raynor, and Hume-Rothery2 found a similar phase in binary aluminum-manganese alloys and, as a result of their experiments, concluded that the G phase was a metastable phase existing in the aluminum-manganese system. This phase was stabilized by the addition of chromium. The constitutional work of Raynor and Little,' although showing the existence of the G phase in the aluminum-chromium-manganese system, did not establish precisely the composition limits of the phase or the temperature above which the phase became unstable and disappeared from the system. The work described in this paper was undertaken to provide this information. An examination of the previous work' showed that an isotherm at 550°C would provide the required data regarding composition in the shortest possible time, as the (a + G) phase field narrows considerably at higher temperatures. The same work showed that the G phase ceased to exist between 580° and 595°C. A more precise estimate of the transformation temperature would therefore be obtained by annealing selected alloys at successively higher temperatures beginning at 580°C. EXPERIMENTAL PROCEDURE 1) Materials Used—The experimental alloys were prepared from four master alloys containing 15.00 w pct Cr, 15.28 wt pct Cr, 19.80 wt pct Mn, and 19.38 wt pct Mn which were made from super-purity aluminum, electrolytic chromium, and electrolytic manganese. The aluminum was of 99.996 pct purity, the principal impurities being copper, iron, and silicon. The chromium and manganese were 99.9 pct pure, the principal impurities being antimony, calcium, and magnesium. 2) Preparation of the Experimental Alloys—The alloys were prepared in 20-g quantities by melting together the requisite amounts of master alloy and aluminum in an alumina-lined crucible and, after thorough stirring with an alumina rod, cast into a cold copper mold to give ingots 1/4 in. in diam and 3 in. in length.

Jan 1, 1960

By R. S. Silo

A new process for leaching oxidized copper ore (CuO) is presented. Its principle advantage is that it requires low cost raw materials. For large operations the only materials used are sodium chloride (NaCl) and calcium carbonate (CaCO3). In those operations of medium size, sulfur, which is abundant in the North of Chile, is used. However the process may also be applied to small copper plants provided low cost sulfuric acid is available as a substitute for sulfur. That is, it may be applied to those small capacity plants where large additional installations for the regeneration of the leaching solution are not needed. The method is comprised of six stages, namely: Crushing, Leaching, Washing of the Solution, Precipitation, Regeneration of the Leaching Solution, and Fusion. A flow diagram for this process in a large or medium-sized plant is given. LEACHING This process requires hydrochloric acid as the leaching solution for treating copper ores. This is easily produced from sulfuric acid and sodium chloride as follows: A small excess of NaCl is advisable to avoid the presence of free sulfuric acid. The experiments reported here were performed with 36 grams of HC1 per liter of solution to obtain a free acidity equivalent to 50 gpl of H2SO4 (the usual leaching solution concentration). Hydrochloric acid leaching may be done by either of the usual methods; i.e. percolation or agitation. The method selected depends on the characteristics of the ore. No matter which method is chosen, low pressure air can be used either as an air lift for circulation of the solution, or for agitation of the pulp with "Pachuca" tanks. In either case, there are no problems with respect to oxidation. Leaching by agitation produces good recovery; but at times, the problem of high consumption of leaching solution or the overproduction of grinding slimes which interfere with contact between phases negates this advantage. The percolation method was used in this study. Percolation took place in four 15-liter containers, 11 1/2 in. diam. by 12 in. height, having hemispheric bottoms. Each container was fitted with a wooden bottom having 1/4 in- holes. The air lift was a 3/4 in. plastic tube 10 in. high. Air at 6 psi was supplied from a rotating laboratory compressor. 10 kg of ore were charged to the container and counter-current leaching was used. The leaching solutions were fed through the center pipe in order to use the ascending solutions to reject the air in the charge. The solution circulated through the air lift in order to facilitate the movement according to the increase in density produced by the reaction between the phases present. Specific observations made in this report cannot be generalized because the leaching characteristics are dependent on the nature of the ore used, the method of leaching, and the production of primary or secondary slimes while crushing or leaching.

Jan 1, 1967

By G. B. Walker, S. A. Falconer, S. J. Swainson, H. H. Vogel

During the past few years much interest and attention has been focused on a relatively new method of ore concentration, which utilizes the principles of sink and float and employs as the heavy medium a suspension in water of a finely ground solid, such as galena or ferrosilicon. Although a relatively recent development, much progress has already been made in applying heavy-media separation processes to a considerable number of ores. Eight plants in this country and abroad are now treating approximately 10 million tons of ore annually by heavy-media separation (sink-float) processes, including lead-zinc, lead, iron, garnet, tin and tungsten. At the annual meeting of the A.I.M.E. in 1941, three interesting papers (unpublished) dealing with heavy-media separation (sink-float) processes of ore concentration as practiced in four commercial units in the United States were presented by Victor Rakowsky, Grover Holt, Elmer Isern and Robert Ammon. These papers gave an excellent exposition of the principles of sink and float, as well as the operating practice in two iron-ore-beneficiation plants, the Harrison and the Merritt, of Butler Brothers, in Minnesota; the Central mill of the Eagle Picher Mining and Smelting Co.; and the Mascot mill, of the American Zinc, Lead and Smelting Co. Augmented by pictorial descriptions and a working model demonstrating the processes, these papers evoked a great deal of interest and discussion. In fact, in reporting the high lights of the meeting in the April 1941 issue of Mining and Metallurgy, Professor Taggart made the statement that " preconcentration by heavy suspension was Miss A.1.M.E 1941 so far as milling is concerned." Although to date the greatest application of heavy-media separation from the tonnage point of view has been for the treatment of lead, zinc and iron ores, these processes have a much wider field of usefulness. In this regard, it is to be noted that recently new heavy-media separation plants for treating cassiterite ore and garnet ore have been placed in successful operation. Moreover, numerous other types of ores have been found to respond well to these processes when tested on a semi-commercial scale, and it is expected that in the near future a considerable number of new plants will be erected. In view of the fact that heavy-media separation processes offer such attractive possibilities, particularly now, when the mining industry is being called on for an even larger production than ever before has been attempted, despite shortages of labor and supplies, it was felt that a description of some of the successful separations that have been worked out during the past year in the Ore Dressing Laboratory of the American Cyanamid Co. on a variety of ores of strategic importance would be of interest. The purpose of this paper, therefore, is to present the essential data relating to investigations of heavy-

Jan 1, 1943

By J. J. Gilman

THEORIES of fracture in metals have been based primarily on the dependence of fracture strength on grain size. This dependence was first observed by Masing and Polanyi.l These workers, as well as 0rowan12 and Davidenkov and Wittman,' thought the grain size could be equated with the crack size in the Griffith condition for crack propagation.4 In this way they could account for the observed proportionality between fracture stress and the reciprocal square root of the grain size. The chief results of recent investigations of the fracture strength of polycrystals are summarized in Fig. 1. Low for iron,5 Petch for iron,' Greenwood and Quarrel for zinc, Petch and Zein for zinc,' and Hauser, Landon, and Dorn for magnesium'' have all found that the fracture stress of a polycrystal is proportional to the reciprocal square root of the grain size. Also, they find that, for large grain sizes, the fracture stress lies near the extrapolation of the yield-stress curve determined at small grain sizes; where measurable plastic strain precedes fracture. Low9 has gone a step further and shown that, in Range 1, the fracture stress in tension is almost identical to the yield stress in compression for a given grain size. Homes and Gouzou, 10 and Low also have shown that, in Range 2 of Fig. 1, microcracks form when the yield stress is reached, but they do not cause failure until the stress reaches a much higher value. The fact that yielding always precedes fracture suggests that fracture is induced by plastic flow. A mechanism by which this might occur was first proposed by Zener.11 He pointed out that blocked dislocations would cause stress concentrations which might cause fracture. The blocking would be caused by grain boundaries. This idea has been developed by Eshelby, Frank, and Nabarro,12 by Koehler,13 and by Stroh.14 By means of etchpits blocked dislocations have been observed in brass by Jacquet,15 in zinc by Gilman,16 and in lithium fluoride by Gilman and johnston. The blocked-dislocation theory and the experiments that bear on it have been summarized by Mott.18 One of the strong points of the blocked-dislocation theory is that it can explain the grain-size dependence of the fracture stress in a natural way. However, Low9 has pointed out that the theory is not satisfying when it is considered quantitatively. Gilman10 also has criticized the theory and presented an alternative interpretation of the relation between fracture stress and grain size. Since the blocked-dislocation theory is not the only theory that can explain in the grain-size effect, it is necessary to find other evidence either to support or deny it. In this investigation the following points were studied: 1) If blocked dislocations normally cause fracture, then the fracture stress ought to be very high in the absence of plastic glide. Is it? 2) If dislocations must be blocked in order for metals to fracture, then certain types of grain

Jan 1, 1959

By G. B. Walker, S. J. Swainson, S. A. Falconer, H. H. Vogel

During the past few years much interest and attention has been focused on a relatively new method of ore concentration, which utilizes the principles of sink and float and employs as the heavy medium a suspension in water of a finely ground solid, such as galena or ferrosilicon. Although a relatively recent development, much progress has already been made in applying heavy-media separation processes to a considerable number of ores. Eight plants in this country and abroad are now treating approximately 10 million tons of ore annually by heavy-media separation (sink-float) processes, including lead-zinc, lead, iron, garnet, tin and tungsten. At the annual meeting of the A.I.M.E. in 1941, three interesting papers (unpublished) dealing with heavy-media separation (sink-float) processes of ore concentration as practiced in four commercial units in the United States were presented by Victor Rakowsky, Grover Holt, Elmer Isern and Robert Ammon. These papers gave an excellent exposition of the principles of sink and float, as well as the operating practice in two iron-ore-beneficiation plants, the Harrison and the Merritt, of Butler Brothers, in Minnesota; the Central mill of the Eagle Picher Mining and Smelting Co.; and the Mascot mill, of the American Zinc, Lead and Smelting Co. Augmented by pictorial descriptions and a working model demonstrating the processes, these papers evoked a great deal of interest and discussion. In fact, in reporting the high lights of the meeting in the April 1941 issue of Mining and Metallurgy, Professor Taggart made the statement that " preconcentration by heavy suspension was Miss A.1.M.E 1941 so far as milling is concerned." Although to date the greatest application of heavy-media separation from the tonnage point of view has been for the treatment of lead, zinc and iron ores, these processes have a much wider field of usefulness. In this regard, it is to be noted that recently new heavy-media separation plants for treating cassiterite ore and garnet ore have been placed in successful operation. Moreover, numerous other types of ores have been found to respond well to these processes when tested on a semi-commercial scale, and it is expected that in the near future a considerable number of new plants will be erected. In view of the fact that heavy-media separation processes offer such attractive possibilities, particularly now, when the mining industry is being called on for an even larger production than ever before has been attempted, despite shortages of labor and supplies, it was felt that a description of some of the successful separations that have been worked out during the past year in the Ore Dressing Laboratory of the American Cyanamid Co. on a variety of ores of strategic importance would be of interest. The purpose of this paper, therefore, is to present the essential data relating to investigations of heavy-

Jan 1, 1943

By R. E. Smallman

R. E. Smallman (University of Birmingham, England)—Recently, Tedmon and Ferriss11 have determined the yield stress parameters oi and ky for tantalum by measuring the lower yield stress as a function of grain size 2d and fitting the results to a relationship of the form They report that although ky , which is taken to be a measure of the dislocation locking strength, is small (- 2 to 4 x 106 cgs units) a substantial yield drop is nevertheless observed in a normal tensile test. Niobium gives a similar result,12-14 as pointed out in the original work by Adams et a1.,12 and in order to check this apparent anomaly the yield-stress parameters of electron beam-melted niobium have recently been reanalyzed15 by the Luders strain technique. In this method the strain hardening part of the stress-strain curve is extrapolated to zero plastic strain; the intercept on the preyield portion of the curve is taken to give oi, whilst the difference between oi and the lower yield stress gives kyd-1/2. The results indicate that ky increases with increasing grain size and hence, a plot of vs d-112 yields an apparent ky, which is lower than the true value. A similar effect could account for the small ky found in the relatively pure tantalum used by Tedmon and Ferriss. The variation of ky with grain size shows that dislocations are more strongly locked in coarse-grained specimens than in fine-grained samples. In niobium, this may be attributed to the fact that the dislocation density in the fine-grained material is higher than that found in the coarse-grained samples which are given a sufficiently prolonged anneal to remove any residual substructure and, since the metal contains only a small amount of interstitual impurity, a variation in locking occurs. By contrast, application of both the grain size analysis and the Luders strain method to yield-stress data from commercially pure vanadium containing a large amount of interstitial impurity gives consistent values of oi and ky, with ky independent of grain size and temperature. Electron microscope observations show minor variations in dislocation density from grain size to grain size, but in any case in this material the dislocations are heavily locked with precipitate. On yielding new dislocations are generated and, as a consequence, the importance of any differences in dislocation density between the various specimens of different grain size is considerably reduced. It is perhaps significant that Adams and lannucci,16 working with a grade of tantalum containing a higher interstitial content than that used by Tedmon and Ferriss, prepared the specimens of different grain size by annealing in the temperature range 1500" to 2000° C to minimize any differences in dislocation structure, and found that ky had a value of 1.04 x 107 cgs units, independent of testing temperature. Such behavior is consistent with the dislocations being locked by carbide precipitates so that the generation of free dislocations is an athermal process. The recent work of Gilbert et al.17 also shows that in tantalum there is no significant variation of ky with grain size provided it contains 150 ppm of oxygen. In this case, however, the dislocations are not locked by precipitate and ky is temperature dependent. C. S. Tedmon and D. P. Ferriss (authors' reply)— We would like to thank Dr. Smallman for his interesting comments and discussion to our paper, "The Dependence of Yield Stress on Grain Size for Tantalum and a 10 pct W-90 pct Ta Alloy".18 It was suggested that perhaps the relatively small values obtained by us for ky of tantalum could be attributed to the same cause that accounts for the apparently small values of ky that result when it is determined by the Luders Strain technique. Since our values were obtained by plotting the lower yield stress vs the reciprocal of the square root of the grain size, it is not clear how this could be the case. The values of ky in this experiment have been calculated, using the Luders strain technique. With this method, values for ky on the order of 2 x 105 to 5 x lo6 cgs units were obtained. In spite of this rather large variation, the magnitudes are still small, and there appeared to be no good correlation between ky and the grain size or the yield stress, probably because of the difficulty in accurately extrapolating the work-hardening portion of the curve back to zero plastic strain. As was shown in the original data,18 there was little work hardening in any of the curves, at any temperature. In his discussion, Dr. Smallman also points out how ky has been observed to increase with increasing grain size, when determined by the Luders strain technique. There are at least two possible explanations for this. In the first case, if it is assumed that the bulk of the interstitial impurities are concentrated at the grain boundaries, then, of course, the available grain boundary area would decrease with increasing grain size, thus presenting less area for the interstitials, which would then presumably increase the concentration within the grains, thereby increasing the locking of the dislocations. In the second case, the increase in ky with increasing grain size would be attributed to the nature of the grain boundary itself. One of the several ways of deriving the Hall-Petch equation19 is based on the stress concentration arising from a pile-up of dislocations at the boundary. The ability of the stress concentration to unlock a source in a neighboring grain would depend on the strength of the grain boundary. As is well-known, the nature and struc-

Jan 1, 1963

By W. B. Agocs

IN August 1954 a low altitude test geophysical survey was made in the Green Pond area of Morris County, New Jersey, with a Gulf Research and Development Co. Model II total magnetic field variation magnetometer mounted in a Sikorsky S-55 helicopter. The test was made in this area to compare the results of a high precision, very low altitude magnetometer survey with an existing ground magnetic survey in this area having known magnetite concentrations, so that the method could be used in areas of difficult access for the detailing of airborne magnetometer anomalies of interest in place of ground surveys. The load capacity of the Sikorsky S-55 permitted installation of a recording scintillation counter so that a radioactivity survey would be made simultaneously with the magnetometer survey. The area surveyed is located at approximately 41°00'N and 74o28'W, just south and east of the town of Green Pond, N. J. The outstanding topographic feature of the region is Copperas Mountain, a well defined ridge, maximum elevation 1222 ft, which runs the entire length of the survey. The lowest point in the survey, 810 ft, is in the extreme eastern corner. Topography of the area is shown in Fig. 1. The three major rock units outcropping in the area are all metamorphic: the Pochuck gneiss, which has been divided into two metamorphic facies; the Byram gneiss; and the Green Pond conglomerate. The relative ages of the Pochuck and Byram formations, both pre-Cambrian, are in doubt, but it is believed that the Pochuck is the older of the two.' The Green Pond conglomerate is Silurian.' Distribution of the outcrops and mine locations is shown in Fig. 1. Two facies of the Pochuck gneiss can be distinguished locally—the Copperas Mountain and Kitchell members. The Copperas Mountain member is a hornblende gneiss, and all the mines and prospects in the area are in this unit. The Kitchell is a quartz-plagioclase feldspar gneiss. The Byram gneiss is a relatively nonresistant valley formation which is high in the potash feldspar. The Green Pond conglomerate is a well indurated quartzite-conglomerate which forms the Copperas Mountain and the Green Pond Mountain's ridge to the north. It overlies the gneisses with a strong angular discordance that may be a fault. The geologic structure of the Green Pond area is relatively uncomplicated. The foliation planes of the gneisses dip steeply to the southeast, and the Green Pond conglomerate dips steeply to the northwest. Additional faulting in the area is indicated at the contact between the Kitchell member of the Pochuck and the Byram along the base of the topographic spur extending to the southeast from Copperas Mountain. The magnetite mines of Pardee, Winter, Davenport, Green Pond, Copperas, and the Bancroft shaft are described by Bayleyl and Stampe2.' The ore is in the Copperas Mountain member of the Pochuck gneiss. The magnetite veins are 10 to 50 ft wide and up to 300 ft long, dipping to the southeast at angles ranging from 40" to 75". The locations of these mines are shown in Fig. 1. Dip Needle Survey: The dip needle survey shown in Fig. 2 was taken from a U. S. Bureau of Mines Report of Investigations." The figure numbers below the local, individual map area outlines refer to the figures in the aforementioned reports which were not contoured. The area of the dip needle survey was confined almost exclusively to the outcrops of the Pochuck gneiss. The separation between survey profiles was 100 ft and the distance between stations on the profiles was 25 ft in highly anomalous zones to 100 ft in magnetically flat areas. A total of 16 1/2 miles of traverse was surveyed over an area of approximately 1/2 sq mile with 2050 stations. The magnitude of the magnetic anomalies is difficult to determine due to the lack of information concerning the type of dip needle used and the procedure followed in making the dip needle survey. This latter would include the method of "zeroing" the dip needle and the procedure of reading at the stations, whether on the swing or statically. Calibrations made of the Gurley dip needle, Lake Superior type, show a static sensitivity of 385 gamma per degree in the range from —25" to +35o, corresponding to a variation in the total field of —9600 gamma to +13500 gamma in a total field of 57000 gamma, inclination 72". The sensitivity increases to 16 gamma per degree from a deflection of 60" to 76", and from 76" to 172" the sensitivity decreases continuously to a low of 260 gamma per degree. From the above it may be seen that it is difficult to assign an arbitrary sensitivity for the dip needle used on this survey. However, an estimated value of 100 gamma per degree may be assigned. On this basis, the majority of the magnetic anomalies, whose deviation is +20°, would be 2000 gamma. Locally, west and northwest of the Pardee mine the magnetic anomaly is +50°, or 5000 gamma; in the Green Pond mine area deviations of +75" are observed that would correspond to anomalies of 7500 gamma. The areal extent and width of the dip needle magnetic anomalies is comparable to profile and station spacing. Hence it is concluded that part of the detail may be due to control, and the probable cause of the magnetic anomalies is at or near surface exposures of magnetite concentrations in the form of veinlets and disseminations whose locations correspond to the local magnetic anomalies. On the basis of the magnetics, none of the magnetite concentra-

Jan 1, 1956

By R. C. Gifkins, K. U. Snowden

The value of the index n in power ktivs for the stress sensitivity of minimum creep rale at lead is derived front results drawn from lite literature and from previously unpublished nork on commercial (99.99 pel) and high-purity (99.999 pel) lead polycryslalline and hi crystal specimens. In tests al 0.5Tm (22 to 50'C) for slvesses below 250 psi, n fulls to mily for poly-cr,yslullirle specimens, single crystals, and bicrystals, and toy grain boundary sliding in bicrystals. Between 250 and 500 psi there is a tyansilion range and, for the polycrystalline specimens al least, u high-stress regime for 500 to 1500 psi where n is 5 or 6. These results are such that none of the suggested stress taws can he used to extrapolate to very loir stresses. Meclianisms for deformation in Ike grains and toy grain boundary sliding in the low-strcss regime are outlined. In particular, the mechanism for grain boundary sliding involves sliding controlled by diffusion from tensile to compressire Ledges. predictions based on this model give promising numerical agree-nicul with experiment. II is suggested that the mechanism for grain boundary sliding may he important in other circumstances, e.g., in creep of ceramic materials or superplaslicity, because it can operate with lille or no dislocation aclirity. WhEN the stress dependence of secondary creep rate is represented by a power law the values taken by the stress exponent n are found to vary between 1 and 7, see, c.g., Garofalo.' In Eq. 1 11 u is the applied stress and A a constant. The case for accepting values of v = 1 rests principally upon tests at high temperatures (>0.9Tm) and there have only been isolated tests at lower temperatures (rather than plots of creep rate against stress) for which the creep rates are such that some form of Nabarro-Herring creep with n = 1 is applicable. Hanson5 and Greenwood and cole6 plotted creep rate against stress for tests made in the vicinity of 0.5Tw, and found a "creep yield", so that below a certain low stress the creep rate was linearly related to stress: these observations appear to have been subsequently ignored. Various models have been proposed which agree with a large body of experimental results in which n equals -5 at high stresses (e.g., weertman7 and McLean8). Various alternatives to Eq. [1] have been proposed principally as a means of unifying creep data, but sometimes, it seems, in order to obviate the necessity for assuming a series of regimes of deformation associated with the various values of n; further refer- ence to these will be made in the section on stress laws. This paper calls attention to extensive results which show n = 1 for the creep of lead at room temperature (0.5 T,). RESULTS Fig. 1 is a composite diagram based on figures in the literature6,9,10 with additional results obtained by the present authors and their colleagues11,12 in the course of a number of investigations not directly concerned with stress sensitivity. In Fig. 1 In creep rate is plotted against In stress. The curves show results for two kinds of material. Lead I is of commercial purity (99.99 pct Pb) and lead IT a specially refined material, hydrogen-purified to remove oxygen; it contains 99.999 pct Pb. Curve A is for lead I in polycrystalline form (grain diameter 0.02 to 0.05 cm) at room temperature (22' to 26°C). Curve B1 is for lead I, polycrystalline, tested at 50C. Curve B2 is for lead 11, polycrystalline (grain diameter 0.02 cm), tested at room temperature (22 O- Curves C to F relate to tests made of bicrystals of lead 11: all of the same nominal orientation ("Y" in Ref. 12). Curves C and V are for creep within the component crystals of the bi crystals at 22°C (AB and CD in Fig. 2). Curve E is for creep measured in a gage straddling the boundary, approximately 0.15 mm either side (BC in Fig. 2). Curve F shows rates of grain boundary sliding (as distinct from strain rates in the other curves), obtained by averaging the offsets of six marker lines on the bi-crystal boundaries. The principal feature of the results is that the stress sensitivity falls into two distinct regimes, according to whether the stress is below approximately 250 or above 500 psi (there is a transitional range between 250 and 500 psi). The new result is that below -250 psi two of the curves (A and BI) give a value of n 1, and the other curves also drop below n - 2 to -1.5 but do not extend to low enough stresses to show clear evidence of n 1. At very high stresses the curves tend to give values of n - 6, as previously determined in other investigations. Curve R2 for the high-purity lead in polycrystalline form at room tenlperature almost merges with B, and thus gives new significance to the values for stresses of 150 and 200 psi; previously'3 these points had seemed to fall away from the curve of slope -3, but they now can be seen as almost completing a transition to n = 1. It should be noted that there was originally considerable apparent scatter in the results for the high-purity lead. However, this was found to be associated with annealing conditions or variations in residual content of oxygen and curve B2 was constructed using the highest rate (i .e., the rate for the purest lead) determined for each stress during the course of various investigations over the years: altogether, some forty tests were used in constructing curve R2.

Jan 1, 1968